US20200013580A1 - Electron microscope with improved imaging resolution - Google Patents

Electron microscope with improved imaging resolution Download PDF

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US20200013580A1
US20200013580A1 US16/453,699 US201916453699A US2020013580A1 US 20200013580 A1 US20200013580 A1 US 20200013580A1 US 201916453699 A US201916453699 A US 201916453699A US 2020013580 A1 US2020013580 A1 US 2020013580A1
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electron microscope
specimen
microscope according
elongate beam
beam conduit
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Alexander Henstra
Pleun Dona
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FEI Co
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FEI Co
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Publication of US20200013580A1 publication Critical patent/US20200013580A1/en
Priority to US18/171,750 priority Critical patent/US20230207254A1/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/04—Arrangements of electrodes and associated parts for generating or controlling the discharge, e.g. electron-optical arrangement or ion-optical arrangement
    • H01J37/09—Diaphragms; Shields associated with electron or ion-optical arrangements; Compensation of disturbing fields
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B21/00—Microscopes
    • G02B21/36—Microscopes arranged for photographic purposes or projection purposes or digital imaging or video purposes including associated control and data processing arrangements
    • G02B21/361—Optical details, e.g. image relay to the camera or image sensor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/04—Arrangements of electrodes and associated parts for generating or controlling the discharge, e.g. electron-optical arrangement or ion-optical arrangement
    • H01J37/10—Lenses
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B21/00—Microscopes
    • G02B21/06—Means for illuminating specimens
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B21/00—Microscopes
    • G02B21/24—Base structure
    • G02B21/26—Stages; Adjusting means therefor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/04—Arrangements of electrodes and associated parts for generating or controlling the discharge, e.g. electron-optical arrangement or ion-optical arrangement
    • H01J37/147—Arrangements for directing or deflecting the discharge along a desired path
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/04—Arrangements of electrodes and associated parts for generating or controlling the discharge, e.g. electron-optical arrangement or ion-optical arrangement
    • H01J37/153—Electron-optical or ion-optical arrangements for the correction of image defects, e.g. stigmators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/20—Means for supporting or positioning the object or the material; Means for adjusting diaphragms or lenses associated with the support
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/22—Optical, image processing or photographic arrangements associated with the tube
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/22—Optical, image processing or photographic arrangements associated with the tube
    • H01J37/226—Optical arrangements for illuminating the object; optical arrangements for collecting light from the object
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/244—Detectors; Associated components or circuits therefor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/02—Details
    • H01J2237/026—Shields
    • H01J2237/0264—Shields magnetic
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/02—Details
    • H01J2237/026—Shields
    • H01J2237/0268—Liner tubes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/153—Correcting image defects, e.g. stigmators
    • H01J2237/1534—Aberrations

Definitions

  • the invention relates to an Electron Microscope comprising:
  • the invention also relates to a method of using such an Electron Microscope.
  • Electron microscopy is a well-known and increasingly important technique for imaging microscopic objects.
  • the basic genus of electron microscope has undergone evolution into a number of well-known apparatus species, such as the Transmission Electron Microscope (TEM), Scanning Electron Microscope (SEM), and Scanning Transmission Electron Microscope (STEM), and also into various sub-species, such as so-called “dual-beam” apparatus (e.g. a FIB-SEM), which additionally employ a “machining” Focused Ion Beam (FIB), allowing supportive activities such as ion-beam milling or Ion-Beam-Induced Deposition (IBID), for example.
  • TEM Transmission Electron Microscope
  • SEM Scanning Electron Microscope
  • STEM Scanning Transmission Electron Microscope
  • STEM Scanning Transmission Electron Microscope
  • an Electron Microscope will comprise at least the following components:
  • FIG. 1 renders a longitudinal cross-sectional elevation view of an embodiment of an EM (in this case, a (S)TEM) in which the present invention is implemented.
  • EM in this case, a (S)TEM
  • FIG. 2A shows a magnified transverse cross-sectional view of part of FIG. 1 .
  • FIG. 2B shows a modified version of the embodiment in FIG. 2A .
  • FIG. 3 is a plot of relative image spread (due to magnetic field noise, and compared to a conventional beam conduit) as a function of log 10 of ⁇ t (skin conductivity ⁇ skin thickness) for an embodiment of the present invention as shown in FIG. 2A , at different beam voltages.
  • FIG. 4 shows a magnified transverse cross-sectional view of an alternative (but related) embodiment to that shown in FIG. 2A / 2 B.
  • a solution that requires cryogenic cooling of “conductive parts of” an EM (such as the iron cores/yokes in magnetic lenses, the beam conduit, etc.) is considered to be highly burdensome.
  • the particle-optical column of an EM is already a tightly packed space in which relatively bulky, ultra-high-precision sub-components are positioned in close proximity to one another within tight tolerances, leaving very little room to spare. It would be an onerous undertaking to try to make additional space in such a set-up for the relatively cumbrous cooling elements/coils/supply lines that would be required to cool large parts of the microscope to cryogenic temperatures.
  • the present disclosure therefore provides a different approach.
  • the inventors decided to replace conventional beam conduit designs by an electrically insulating tube, e.g. comprising a durable ceramic such as Zirconia (ZrO 2 ) or Alumina (Al 2 O 3 ).
  • an electrically insulating tube e.g. comprising a durable ceramic such as Zirconia (ZrO 2 ) or Alumina (Al 2 O 3 ).
  • ZrO 2 Zirconia
  • Al 2 O 3 Alumina
  • a (grounded) skin of electrically conductive material such as a metallic film—which should be relatively thin/resistive, so that it itself does not become a significant harbor/source for parasitic currents.
  • the product ⁇ t of skin (electrical) conductivity ⁇ and skin thickness t can play an indicative role, and there tends to be a general preference for relatively small values of ⁇ t.
  • ⁇ t skin (electrical) conductivity
  • t skin thickness
  • the term “electrically insulating material” can also include materials that might traditionally be considered as being semiconductors.
  • SiC is a ceramic material that is conventionally labelled as being a semiconductor; however, its electrical resistivity is ⁇ 10 6 ⁇ /cm—which makes it about 10 16 times less conductive than aluminum, which has a resistivity of ⁇ 10 ⁇ 10 ⁇ /cm.
  • the electrical resistivities of Quartz, Alumina and Zirconia are ⁇ 10 16 , 10 14 and 10 9 ⁇ /cm, respectively.
  • an electrical insulator is a material in which there is (basically) no free transport of (conduction) electrons, usually due to the presence of a relatively large band gap in such materials.
  • the Electron Microscope as defined herein is characterized in that at least a longitudinal portion of said beam conduit extends at least through said aberration corrector and is comprised of an aggregate composite material comprising:
  • the beam conduit is comprised of an aggregate composite material comprising intermixed electrically insulating material and electrically conductive material.
  • an aggregate composite material comprising intermixed electrically insulating material and electrically conductive material.
  • suitable examples of component materials include:
  • One way of achieving such a composite is to intermix conductive material (e.g. in the form of particles or fibers) in a matrix of insulating material (e.g. in the form of green ceramic material); alternatively, one can start with a conductive material and “temper” its conductivity by intermixing an insulating material therein.
  • the additive in question may, for example, be included in the receptive bulk material using a process such as diffusion or ion implantation, or by physical mixing of granulates, for instance.
  • the skilled artisan will be able to determine the relative quantities of different materials to be mixed in order to achieve an aggregate composite with a given bulk resistivity, and/or he can purchase pre-made products.
  • aggregate composite materials as referred to herein are commercially available from firms such as Poco Graphite, Inc., in Decatur, Tex., USA. They are sometimes referred to as “ESD” materials, because of their suitability to mitigate electrostatic discharge issues. Other terms that are sometimes used for such materials include “electro-ceramics” and “granular metals”.
  • a trajectory extending between the specimen plane (specimen holder) and the aberration corrector is a trajectory extending between the specimen plane (specimen holder) and the aberration corrector.
  • the present invention Using the present invention, one can achieve excellent STEM image resolution values of, for example, 30 pm at a beam voltage of 300 kV, and 60 pm at a beam voltage of 60 kV, in both cases for a beam half opening angle of 50 mrad, and without having to resort to cumbersome cryogenic cooling as set forth in the abovementioned PRL journal article.
  • the invention typically allows image spread caused by Johnson-Nyquist noise to be reduced by a factor of the order of about 10-15.
  • U.S. Pat. No. 3,787,696 A and DE 30 10 376 A1 disclose liner tubes for use in scanning and/or focusing coils.
  • U.S. Pat. No. 3,634,684 A also uses a liner tube for a scanning coil.
  • the liner tubes are used to counter Eddy currents originating from the high-frequency magnetic flux originating from the scanning.
  • JP H03 22339 A discloses an aberration corrector with an electrically conductive inner skin and an electrically isolating outer tube.
  • the electrically conductive inner skin is required to apply a desired voltage to the liner tube and to keep the specimen grounded.
  • FIG. 1 (not to scale) is a highly schematic depiction of an embodiment of an EM M in which the present invention is implemented; more specifically, it shows an embodiment of a TEM/STEM (though, in the context of the current invention, it could just as validly be an SEM, for example).
  • a vacuum enclosure V which can be evacuated by a schematically depicted vacuum pump assembly V′.
  • an electron source 4 produces a beam B of electrons that propagates along an electron-optical axis B′ and traverses an illuminator system (electron beam column) 6 , serving to direct/focus the electrons onto a chosen part of a specimen S (which will generally be (locally) thinned/planarized).
  • a deflector 8 which (inter alia) can be used to effect scanning motion of the beam B.
  • the vacuum enclosure V will generally “hug” the axis B′, taking the form of a relatively narrow elongate beam conduit B′′ (e.g. of the order of ca. 0.5 cm in diameter) through (at least) the illuminator 6 , but widening out where necessary to accommodate certain structures (such as the items H, 26 , 30 , 32 , and 34 discussed below, for example).
  • the specimen S is held on a specimen holder H that can be positioned in multiple degrees of freedom by a positioning device/stage A, which moves a cradle A′ into which holder H is (removably) affixed; for example, the specimen holder H may comprise a finger that can be moved (inter alia) in the XY plane (see the depicted Cartesian coordinate system), with motion parallel to Z and tilt about X/Y also typically being possible.
  • Such movement allows different parts of the specimen S to be illuminated/imaged/inspected by the electron beam B traveling along axis B′ (in the Z direction), and/or allows scanning motion to be performed as an alternative to beam scanning.
  • the specimen holder H can be maintained at a cryogenic temperature using a (schematically depicted) temperature control assembly T; this may, for example, comprise a thermally conductive (e.g. metallic) wick that is thermally connected to the holder H and is immersed in a bath of cryogen, or a pipe system carrying a circulating cryogen, for example.
  • a thermally conductive (e.g. metallic) wick that is thermally connected to the holder H and is immersed in a bath of cryogen, or a pipe system carrying a circulating cryogen, for example.
  • the electron beam B will interact with the specimen S in such a manner as to cause various types of “stimulated” radiation to emanate from the specimen S, including (for example) secondary electrons, backscattered electrons, X-rays and optical radiation (cathodoluminescence).
  • various types of “stimulated” radiation including (for example) secondary electrons, backscattered electrons, X-rays and optical radiation (cathodoluminescence).
  • these radiation types can be nominally detected with the aid of analysis device 22 , which might be a combined scintillator/photomultiplier or EDX (Energy-Dispersive X-Ray Spectroscopy) module, for instance; in such a case, an image could be constructed using basically the same principle as in a SEM.
  • an imaging system projection lens 24
  • this imaging system 24 can focus the transmitted electron flux onto a fluorescent screen 26 , which, if desired, can be retracted/withdrawn (as schematically indicated by arrows 26 ′) so as to get it out of the way of axis B′.
  • An image or diffractogram of (part of) the specimen S will be formed by imaging system 24 on screen 26 , and this may be viewed through viewing ports 28 a , 28 b located in suitable parts of the walls of enclosure V/cabinet 2 .
  • the retraction mechanism for screen 26 may, for example, be mechanical and/or electrical in nature, and is not depicted here.
  • controller 20 is connected to various illustrated components via control lines (buses) 20 ′.
  • This controller 20 can provide a variety of functions, such as synchronizing actions, providing setpoints, processing signals, performing calculations, and displaying messages/information on a display device (not depicted).
  • the (schematically depicted) controller 20 may be (partially) inside or outside the cabinet 2 , and may have a unitary or composite structure, as desired.
  • the interior of the enclosure V does not have to be kept at a strict vacuum; for example, in a so-called “Environmental TEM/STEM”, a background atmosphere of a given gas is deliberately introduced/maintained within the enclosure V.
  • the microscope M can comprise one or more aberration correctors 40 , each of which comprises a multipole lens assembly that is configured to mitigate spherical (Cs) and/or chromatic (Cc) aberration.
  • Cs spherical
  • Cc chromatic
  • the depicted corrector 40 in the illumination system 6 might be a Cs corrector
  • the corrector 40 in the imaging system 24 might be a combined Cs-Cc corrector.
  • beam conduit B′′ comprises a metallic pipe.
  • this basic structure has been modified over at least part of the length (along the Z axis) of the beam conduit B′′.
  • FIG. 2A which shows a magnified transverse cross-sectional view of part of the beam conduit B′′ of FIG. 1 , it is seen that, according to the invention, at least a (longitudinal) portion of beam conduit B′′ has a composite form comprising:
  • FIG. 2B shows a modified version of the situation in FIG. 2A , in which an empty gap 51 exists between outer tube 50 and inner skin 52 .
  • the gap 51 is evacuated to (substantially) the same vacuum level as the interior space of skin 52 , so that there is (substantially) no radial pressure differential across the skin 52 ; conversely, if the interior of skin 52 is at a non-vacuum pressure (e.g. during manufacture, transport, maintenance, etc.), gap 51 is also held at (substantially) this same pressure.
  • a non-vacuum pressure e.g. during manufacture, transport, maintenance, etc.
  • ⁇ t in the form of radial struts, or connected extremities, for instance; it can thus also be described as a sleeve or hose, for example.
  • the illustrated structure also applies/exploits the insights of the current disclosure if skin 52 has a relatively small value of ⁇ t, e.g. ⁇ t ⁇ 0.1 or ⁇ 0.01, for instance.
  • a composite beam conduit structure according to the disclosure and such as that illustrated in FIG. 2A can be manufactured in various ways. For example:
  • tube 50 is pre-formed (e.g. cast or rolled) in a cylindrical shape, and skin 52 is then deposited on its inside surface.
  • V skin ( ⁇ 0 ⁇ t 2 ) ⁇ 1 . (3.1)
  • ⁇ 0 is the permeability of vacuum.
  • Equations for the low frequency variation of the magnetic field are of the form:
  • equation (3.7) can be approximated by:
  • ⁇ r ⁇ m ⁇ d 2 ⁇ r ⁇ dt 2 - e ⁇ v ⁇ ⁇ B ⁇ ⁇ ( z , t ) . ( 3.1 ⁇ .1 )
  • ⁇ r 1+U e/mc 2 .
  • the correlation function for the magnetic field is allowed to vary with frequency, i.e. A n (z) and ⁇ are assumed to be frequency-dependent.
  • ⁇ ⁇ 2 ⁇ ⁇ 2 ⁇ L U r ⁇ ⁇ 0 ⁇ ⁇ dv ⁇ ⁇ B ⁇ 2 ⁇ ( v ) ⁇ ⁇ ⁇ - ⁇ ⁇ ⁇ dz ⁇ ⁇ e i ⁇ ⁇ 2 ⁇ ⁇ ⁇ ⁇ vz / v ⁇ ⁇ A n ⁇ ( z ; v ) , ( 3.1 ⁇ .2 )
  • Equation (3.12) then leads to:
  • ⁇ ⁇ 2 ⁇ ⁇ 2 ⁇ L U r ⁇ ⁇ 0 ⁇ ⁇ dv ⁇ ⁇ B ⁇ 2 ⁇ ( v ) ⁇ ⁇ ⁇ ⁇ ( v ) ⁇ e - ⁇ ⁇ [ ⁇ ⁇ ( v ) ⁇ v / v ] 2 . ( 3.1 ⁇ .3 )
  • FIG. 4 shows a magnified transverse cross-sectional view of an alternative embodiment to that shown in FIG. 2 (A and/or B).
  • the laminate composite of FIG. 2 has been replaced by an aggregate composite material 54 comprising intermixed electrically insulating material and electrically conductive material, thus producing a “hybrid” material with a lower conductivity ⁇ than that of the skin 52 in FIG. 2 .
  • the conduit B′′ has a wall thickness t w , which is larger than the skin thickness t in FIG. 2 .
  • the product ⁇ t w is relatively small, e.g. ⁇ 0.01 ⁇ ⁇ 1 , or even ⁇ 0.001 ⁇ ⁇ 1 .

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Engineering & Computer Science (AREA)
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  • Analysing Materials By The Use Of Radiation (AREA)
  • Electron Sources, Ion Sources (AREA)
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US20230127466A1 (en) * 2020-03-02 2023-04-27 National Institute For Materials Science Device for observing permeation and diffusion path of observation target gas, observation target gas measuring method, point-defect location detecting device, point-defect location detecting method, and observation samples
DE102022124933A1 (de) * 2022-09-28 2024-03-28 Carl Zeiss Multisem Gmbh Vielstrahl-Teilchenmikroskop mit verbessertem Strahlrohr
DE102023101628A1 (de) 2023-01-24 2024-07-25 Carl Zeiss Microscopy Gmbh Teilchenstrahlmikroskop

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US11437216B2 (en) 2020-12-31 2022-09-06 Fei Company Reduction of thermal magnetic field noise in TEM corrector systems
CN119470525A (zh) * 2025-01-15 2025-02-18 华东师范大学 一种在原位电子显微镜中测试电子元器件性能的方法

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US20230207254A1 (en) 2023-06-29
EP3594987A3 (en) 2020-12-23
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EP3594987A2 (en) 2020-01-15
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